Manufacturing methods for the production of carbon materials

Abstract

The present application is generally directed to activated carbon materials and methods for making the same. The disclosed methods comprise rapidly freezing synthetically prepared polymer gel particles. The methods further comprise drying, pyrolyzing, and activating steps to obtain an activated carbon material of high porosity. The disclosed methods represent viable manufacturing processes for the preparation of activated carbon materials.

1. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises immersing the polymer gel particles in a liquid having a temperature below about −10° C. 
     
     
       2. The method of  claim 1 , wherein rapidly freezing the polymer gel particles comprises immersing the polymer gel particles in a liquid having a temperature below about −30° C. 
     
     
       3. The method of  claim 1 , wherein the polymer gel particles are generated by grinding or milling the polymer gel. 
     
     
       4. The method of  claim 1 , wherein the liquid is liquid nitrogen. 
     
     
       5. The method of  claim 1 , wherein the liquid is ethanol. 
     
     
       6. The method of  claim 1 , wherein the polymer gel particles have an average particle size of less than about 30 mm. 
     
     
       7. The method of  claim 6 , wherein the polymer gel particles have an average particle size of about 0.5 mm to about 10 mm. 
     
     
       8. The method of  claim 1 , wherein the polymer gel particles are immersed in the liquid at a rate of about 5 grams/min. 
     
     
       9. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises:
 a) admixing the polymer gel particles with a cold solid; 
 b) admixing the polymer gel particles with a gas having a temperature below about −10° C.; or 
 c) grinding or milling the polymer gel in the presence of a cold solid. 
 
     
     
       10. The method of  claim 9 , wherein the cold solid is solid carbon dioxide. 
     
     
       11. The method of  claim 9 , wherein the gas is nitrogen. 
     
     
       12. The method of  claim 9 , wherein the cold solid is solid carbon dioxide. 
     
     
       13. A method for making frozen polymer gel particles, the method comprising rapidly freezing polymer gel particles, wherein the polymer gel particles have been generated from a polymer gel, and wherein the polymer gel has been prepared by reaction of one or more polymer precursors, wherein rapidly freezing the polymer gel particles comprises:
 a) contacting the polymer gel particles with an atomized liquid having a temperature below about −10° C.; 
 b) contacting sprayed droplets comprising the polymer gel particles with a cold medium having a temperature below about −10° C. to obtain frozen droplets comprising the frozen polymer gel particles; or 
 c) rapidly pulling a vacuum on the polymer gel particles. 
 
     
     
       14. The method of  claim 13 , wherein rapidly freezing the polymer gel particles comprises contacting the polymer gel particles with an atomized liquid having a temperature below about −30° C. 
     
     
       15. The method of  claim 13 , wherein the atomized liquid is liquid nitrogen. 
     
     
       16. The method of  claim 13 , wherein the cold medium has a temperature below about −30° C. 
     
     
       17. The method of  claim 13 , wherein the sprayed droplets comprise a suspension of the polymer gel particles. 
     
     
       18. The method of  claim 13 , wherein the polymer gel particles comprise polymer gel having a viscosity of less than about 1000 cP. 
     
     
       19. The method of  claim 13 , wherein the polymer gel particles comprise incompletely polymerized polymer gel. 
     
     
       20. The method of  claim 19 , wherein polymerization of the polymer gel is completed after the sprayed droplets are contacted with the cold medium (i.e. after the freezing step). 
     
     
       21. The method of  claim 20 , further comprising lyophilizing the frozen droplets to obtain freeze-dried particles and completing the polymerization reaction within the freeze-dried particle. 
     
     
       22. The method of  claim 20 , further comprising completing the polymerization of the polymer gel within the frozen droplets. 
     
     
       23. The method of  claim 13 , wherein the sprayed droplets further comprise microspheres comprising the polymer gel particles. 
     
     
       24. The method of  claim 23 , wherein the microspheres comprise an emulsion selected from a water-in-oil (w/o) emulsion, oil-in-water (o/w) emulsion, oil-in-water-oil (o/w/o) emulsion, water-in-oil-in-water (w/o/w) emulsion, and water-in-oil-in-oil (w/o/o) emulsion. 
     
     
       25. The method of  claim 24 , wherein the emulsion comprises a surfactant selected from non-ionic, cationic, non-ionic polymeric, and non-ionic polymeric fluorinated surfactants. 
     
     
       26. The method of  claim 13 , wherein the cold medium is liquid nitrogen or ethanol. 
     
     
       27. A polymer cryogel comprising less than about 1000 ppm of t-butanol, wherein the polymer cryogel has a tap density of between about 0.15 cc/g and about 0.25 cc/g.